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Z. Voitko et al.
2 Experimental
2.1 Synthesis of HA
Synthesis of the HA was implemented as follows. Initially, a sucrose solution with the
concentration of 0.1 mol/dm
3 was prepared, to which 2 g of calcium oxide was added
and left for 7 days to form the solution of calcium saccharate. A stoichiometrically
calculated amount of ammonium hydrophosphate was added to the obtained calcium
saccharate solution and stirred. After that, ammonia water (25%) was added dropwise
under stirring to pH 10. The procedure was carried out at 313–323 K. After the
addition of all reagents, the mixture was stirred for another 1 h and left for 7 days
aging. Thereafter, the suspension was filtered, and the resulting precipitate was dried
at 353 K.
2.2 Synthesis of HA–Collagen Composite
Synthesis of the HAP–collagen composite was provided in the same way as HA
synthesis, but collagen was also added together with ammonium hydrophosphate.
2.3 Synthesis of HA–Collagen–Alginate Composite
For the synthesis of the HA–collagen–alginate composite, 1%wt alginate solution
was first prepared. After obtaining a viscous solution of alginate, an HA–collagen
composite was added to it. The obtained suspension was added dropwise to the 5%wt
CaCl 2 solution. As a result, the balls which contained HA–collagen–alginate were
formed. The resulting balls were separated from the solution and air-dried.
2.4 X-Ray Analysis
XRD (X-ray diffraction) measurements of the HA and HA–collagen samples were
conducted using X-ray diffractometer Ultima IV Rigaku with CuKa radiation [13,
14]. Samples were automatically analyzed by the PDXL software package using
ICDD/PDF-2 database (standard card of HA is ICDD 9002214).
The diffraction patterns of the pure HA and HA–collagen composite are shown
in Fig. 2. Both samples contained the crystalline phase of 100% hydroxyapatite. The
crystallite size was 5.3 nm for the HA sample and 2 nm for the HA–collagen sample.
Therefore, in both cases, nanocrystalline HA was obtained, but in the presence of
Z. Voitko et al.
2 Experimental
2.1 Synthesis of HA
Synthesis of the HA was implemented as follows. Initially, a sucrose solution with the
concentration of 0.1 mol/dm
3 was prepared, to which 2 g of calcium oxide was added
and left for 7 days to form the solution of calcium saccharate. A stoichiometrically
calculated amount of ammonium hydrophosphate was added to the obtained calcium
saccharate solution and stirred. After that, ammonia water (25%) was added dropwise
under stirring to pH 10. The procedure was carried out at 313–323 K. After the
addition of all reagents, the mixture was stirred for another 1 h and left for 7 days
aging. Thereafter, the suspension was filtered, and the resulting precipitate was dried
at 353 K.
2.2 Synthesis of HA–Collagen Composite
Synthesis of the HAP–collagen composite was provided in the same way as HA
synthesis, but collagen was also added together with ammonium hydrophosphate.
2.3 Synthesis of HA–Collagen–Alginate Composite
For the synthesis of the HA–collagen–alginate composite, 1%wt alginate solution
was first prepared. After obtaining a viscous solution of alginate, an HA–collagen
composite was added to it. The obtained suspension was added dropwise to the 5%wt
CaCl 2 solution. As a result, the balls which contained HA–collagen–alginate were
formed. The resulting balls were separated from the solution and air-dried.
2.4 X-Ray Analysis
XRD (X-ray diffraction) measurements of the HA and HA–collagen samples were
conducted using X-ray diffractometer Ultima IV Rigaku with CuKa radiation [13,
14]. Samples were automatically analyzed by the PDXL software package using
ICDD/PDF-2 database (standard card of HA is ICDD 9002214).
The diffraction patterns of the pure HA and HA–collagen composite are shown
in Fig. 2. Both samples contained the crystalline phase of 100% hydroxyapatite. The
crystallite size was 5.3 nm for the HA sample and 2 nm for the HA–collagen sample.
Therefore, in both cases, nanocrystalline HA was obtained, but in the presence of